P
US6943692B2ExpiredUtilityPatentIndex 83

Apparatus and methods for on-line monitoring of fluorinated material in headspace of vial

Assignee: BRISTOL MYERS SQUIBB PHARMA COPriority: Feb 2, 2001Filed: Feb 1, 2002Granted: Sep 13, 2005
Est. expiryFeb 2, 2021(expired)· nominal 20-yr term from priority
Inventors:CASTNER JAMESBOUDREAU LUCRILLING ALLAN
Y10T436/11Y10T436/196666Y10T436/25875Y10T436/115831Y10T436/19Y10T436/113332G01N 2001/2229B07C 5/34G01N 2035/0408G01N 21/13G01N 21/3504
83
PatentIndex Score
27
Cited by
18
References
50
Claims

Abstract

Apparatus and methods for monitoring the presence of an analyte in a closed vial wherein a sample contained within the closed vial is conveyed to an analyzer. The analyzer determines a value of a spectral property dependent on analyte concentration at a position within a headspace formed above the sample within the vial. An indicator is used to compare the measured value of the spectral property with a predetermined limit criteria to determine the presence or absence of the analyte. Vials wherein the presence of the analyte is detected are indicated as product vials whereas vials wherein the absence of the analyte is detected are indicated as rejected vials. The rejected vials are conveyed by a transferrer to a rejected vial station. A first portion of the product vials are conveyed by a sampler to a sample collection station. A second portion of the product vials are conveyed to a labeler.

Claims

exact text as granted — not AI-modified
1. An apparatus for monitoring the presence of an analyte in a closed vial comprising:
 (a) a vial feeding mechanism;  
 (b) a conveyor operatively associated with the vial feeding mechanism for receiving vials from the vial feeding mechanism;  
 (c) an analyzer operatively associated with the conveyor for determining a value of a spectral property between from about 2800 cm −1  and about 2400 cm −1  at a position within headspaces of the vials, the spectral property being dependent on analyte concentration; and  
 (d) an indicator operatively associated with the analyzer and the conveyor for indicating vials wherein the presence of the analyte is detected as product vials and for indicating vials wherein the absence of the analyte is detected as rejected vials.  
 
   
   
     2. The apparatus of  claim 1  comprising a transporter operatively associated with the vial feeding mechanism for receiving vials from the vial feeding mechanism and operatively associated with the conveyor for transferring vials to the conveyor. 
   
   
     3. The apparatus of  claim 2  comprising a first vial counter operatively associated with the transporter for counting the number of vials received by the transporter. 
   
   
     4. The apparatus of  claim 1  comprising a transferrer for receiving vials from the conveyor. 
   
   
     5. The apparatus of  claim 4  comprising a reject station operatively associated with the transferrer for receiving rejected vials from the transferrer. 
   
   
     6. The apparatus of  claim 4  comprising a second vial counter operatively associated with the transferrer for counting the number of vials received by the transferrer. 
   
   
     7. The apparatus of  claim 4  comprising a sampler operatively associated with the transferrer for removing sample collection vials from the transferrer. 
   
   
     8. The apparatus of  claim 7  comprising a third vial counter operatively associated with the sampler for counting the number of vials received by the sampler. 
   
   
     9. The apparatus of  claim 7  comprising a sample collection station operatively associated with the sampler for receiving the sample collection vials from the sampler. 
   
   
     10. The apparatus of  claim 4  comprising a labeler operatively associated with the transferrer for labeling product vials received from the transferrer. 
   
   
     11. The apparatus of  claim 1  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     12. The apparatus of  claim 11  wherein the perfluorocarbon gas comprises perfluoropropane. 
   
   
     13. The apparatus of  claim 1  further comprising a separator situated between the vials on the conveyor, such that the signal from the analyzer does not saturate the indicator as the vials are moved through the optical path of the analyzer. 
   
   
     14. A method for monitoring the presence of an analyte in a closed vial comprising the steps of:
 (a) conveying a sample contained within the closed vial to an analyzer;  
 (b) determining a value of a spectral property between about 2800 cm −1  and about 2400 cm −1  dependent on analyte concentration at a position within a headspace formed above the sample within the vial;  
 (c) comparing the measured value of the spectral property with a predetermined limit criteria to determine the presence of the analyte;  
 (d) indicating vials wherein the presence of the analyte is detected as product vials and indicating vials wherein the absence of the analyte is detected as rejected vials;  
 (e) conveying the rejected vials to a rejected vial station;  
 (f) conveying a first portion of the product vials to a sample collection station; and  
 (g) conveying a second portion of the product vials to a labeler.  
 
   
   
     15. The method of  claim 14  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     16. The method of  claim 15  wherein the perfluorocarbon gas comprises perfluoropropane. 
   
   
     17. The method according to  claim 14 , wherein the analyte comprises a gas selected from the group: fluorocarbon gas and perfluorocarbon gas. 
   
   
     18. The method according to  claim 14 , wherein the analyte comprises a perfluorocarbon gas selected from the group: perfluoromethane, perfluoroethane, perfluoropropane (PFP), perfluorobutane, and perfluoropentane, perfluorobutane, heptafluoropropane and mixtures thereof. 
   
   
     19. The method according to  claim 14 , wherein the sample comprises a fluorinated liquid. 
   
   
     20. The method according to  claim 19 , wherein the fluorinated liquid is selected from the group consisting of: perfluorohexane, perfluoroheptane, perfluorooctane, perfluorononane, perfluorodecane, perfluorododecane, perfluorocyclohexane, perfluorodecalin, perfluorododecalin, perfluorooctyliodide, perfluorooctylbromide, perfluorotripropylamine, perfluorotributylamine, perfluorobutylethyl ether, bis(perfluoroisopropyl) ether and bis(perfluoropropyl) ether, and mixtures thereof. 
   
   
     21. The method according to  claim 14 , wherein the sample comprises a fluorinated liquid selected from the group consisting of: liquid perfluorocarbon and liquid perfluoroether. 
   
   
     22. The method according to  claim 14 , wherein the vial is a plastic vial capable of affording a spectral window through which specific analytes may be detected. 
   
   
     23. A method for monitoring the presence of an analyte in a headspace of a sample vial comprising the steps of:
 (a) performing a first spectral analysis between about 2800 cm −1  and about 2400 cm −1  of an analyte contained within a headspace of a test vial, wherein the concentration of the analyte in the headspace is at a predetermined level;  
 (b) identifying a spectral region containing an absorption peak specific for the analyte in the headspace of the test vial from the first spectral analysis;  
 (c) determining a first intensity for the identified spectral region from the first spectral analysis;  
 (d) performing a second spectral analysis between about 2800 cm −1  and about 2400 cm −1  of gas contained within a headspace of a sample vial containing a sample;  
 (e) determining a second intensity for the identified spectral region from the second spectral analysis;  
 (f) comparing the second intensity with the first intensity to determine the presence of the analyte in the headspace of the sample vial.  
 
   
   
     24. The method of  claim 23  wherein the first and second intensities are determined from a height of the absorption peak. 
   
   
     25. The method of  claim 23  wherein the first and second intensities are determined from an area of the absorption peak. 
   
   
     26. The method of  claim 25  wherein the area of the absorption peak is determined using a partial least squares algorithm of the spectral response or a peak height algorithm. 
   
   
     27. The method of  claim 23  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     28. The method of  claim 27  wherein the perfluorocarbon gas comprises perfluoropropane. 
   
   
     29. An apparatus for quantitatively monitoring the presence of an analyte in a closed vial comprising:
 (a) a vial feeding mechanism;  
 (b) a conveyor operatively associated with the vial feeding mechanism for receiving vials from the vial feeding mechanism;  
 (c) an analyzer operatively associated with the conveyor for determining a value of a spectral property between about 2800 cm −1  and about 2400 cm −1  at a position within headspaces of the vials, the spectral property being dependent on analyte concentration; and  
 (d) an indicator operatively associated with the analyzer and the conveyor for indicating vials wherein the presence of the analyte is measured quantitatively and detected as product vials, and for indicating vials wherein the quantity of analyte measured is different than the analyte in the product vials, these vials are detected as rejected vials.  
 
   
   
     30. The apparatus of  claim 29  comprising a transporter operatively associated with the vial feeding mechanism for receiving vials from the vial feeding mechanism and operatively associated with the conveyor for transferring vials to the conveyor. 
   
   
     31. The apparatus of  claim 30  comprising a first vial counter operatively associated with the transporter for counting the number of vials received by the transporter. 
   
   
     32. The apparatus of  claim 29  comprising a transferrer for receiving vials from the conveyor. 
   
   
     33. The apparatus of  claim 32  comprising a reject station operatively associated with the transferrer for receiving rejected vials from the transferrer. 
   
   
     34. The apparatus of  claim 32  comprising a second vial counter operatively associated with the transferrer for counting the number of vials received by the transferrer. 
   
   
     35. The apparatus of  claim 32  comprising a sampler operatively associated with the transferrer for removing sample collection vials from the transferrer. 
   
   
     36. The apparatus of  claim 35  comprising a third vial counter operatively associated with the sampler for counting the number of vials received by the sampler. 
   
   
     37. The apparatus of  claim 35  comprising a sample collection station operatively associated with the sampler for receiving the sample collection vials from the sampler. 
   
   
     38. The apparatus of  claim 32 , comprising a labeler operatively associated with the transferrer for labeling product vials received from the transferrer. 
   
   
     39. The apparatus of  claim 29  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     40. The apparatus of  claim 39  wherein the perfluorocarbon gas comprises perfluoropropane. 
   
   
     41. The apparatus of  claim 39  further comprising a separator situated between the vials on the conveyor, such that the signal from the analyzer does not saturate the indicator as the vials are moved through the optical path of the analyzer. 
   
   
     42. A method for quantitatively measuring an analyte in a closed vial comprising the steps of:
 (a) conveying a sample contained within the closed vial to an analyzer;  
 (b) determining a value of a spectral property between about 2800 cm −1  and about 2400 cm −1  dependent on analyte concentration at a position within a headspace formed above the sample within the vial;  
 (c) comparing the measured value of the spectral property with a predetermined limit criteria to determine the quantity of the analyte;  
 (d) indicating vials wherein the desired quantity of analyte is detected as product vials and indicating vials wherein the undesired quantity of analyte is detected as rejected vials;  
 (e) conveying the rejected vials to a rejected vial station;  
 (f) conveying a first portion of the product vials to a sample collection station; and  
 (g) conveying a second portion of the product vials to a labeler.  
 
   
   
     43. The method of  claim 42  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     44. The method of  claim 43  wherein the perfluorocarbon gas comprises perfluoropropane. 
   
   
     45. A method for quantitatively monitoring the presence of an analyte in a headspace of a sample vial comprising the steps of:
 (a) performing a first spectral analysis between about 2800 cm −1  and about 2400 cm −1  of an analyte contained within a headspace of a test vial, wherein the concentration of the analyte in the headspace is at a predetermined level;  
 (b) identifying a spectral region containing an absorption peak specific for the analyte in the headspace of the test vial from the first spectral analysis;  
 (c) determining a first intensity for the identified spectral region from the first spectral analysis;  
 (d) performing a second spectral analysis between about 2800 cm −1  and about 2400 cm −1  of gas contained within a headspace of a sample vial containing a sample;  
 (e) determining a second intensity for the identified spectral region from the second spectral analysis; and  
 (f) comparing the second intensity with the first intensity to determine the quantity of the analyte in the headspace of the sample vial.  
 
   
   
     46. The method of  claim 45  wherein the first and second intensities are determined from a height of the absorption peak. 
   
   
     47. The method of  claim 45  wherein the first and second intensities are determined from an area of the absorption peak. 
   
   
     48. The method of  claim 47  wherein the area of the absorption peak is determined using a partial least squares algorithm of the spectral response or a peak height algorithm. 
   
   
     49. The method of  claim 45  wherein the analyte comprises a perfluorocarbon gas. 
   
   
     50. The method of  claim 49  wherein the perfluorocarbon gas comprises perfluoropropane.

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